JP3674858B2 - Method for producing high specific surface area calcium hydroxide particles - Google Patents
Method for producing high specific surface area calcium hydroxide particles Download PDFInfo
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- JP3674858B2 JP3674858B2 JP2002137581A JP2002137581A JP3674858B2 JP 3674858 B2 JP3674858 B2 JP 3674858B2 JP 2002137581 A JP2002137581 A JP 2002137581A JP 2002137581 A JP2002137581 A JP 2002137581A JP 3674858 B2 JP3674858 B2 JP 3674858B2
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Description
【０００１】
【発明の属する技術分野】
高比表面積を有する水酸化カルシウム粒子の製造方法に関するものである。さらに詳しくは、高性能で且つ簡便で経済的な高比表面積を有する水酸化カルシウム粒子の製造方法に関するものである。
【０００２】
【従来の技術】
水酸化カルシウム粒子は一般的に、生石灰（酸化カルシウム）を水と反応させる方法で製造されているが、水中での生石灰の溶解度が高いために結晶成長しやすく比表面積の小さい水酸化カルシウム粒子が生成する。特開２００１−１２３０７１公報では、カルシウムに対して当量以上の水酸化アルカリ金属を含有する水溶液に、水溶性カルシウム塩水溶液を注加して反応させ、熟成する方法が記載されている。しかしながら、上記方法は原料が高価であることおよび副生溶解質を水洗する必要があり且つ生成する粒子が微粒子であるために濾過が困難であるという問題がある。さらに、比表面積も十分に高いものが得られていない。
【０００３】
【発明が解決しようとする課題】
本発明は、従来の水酸化カルシウム粒子の前記した製造方法における問題を克服し、高比表面積を有する水酸化カルシウムを簡便且つ経済的に製造する方法の提供を目的とする。本発明の方法による水酸化カルシウム粒子は、比表面積が大きいので高活性であり、酸中和剤やハロゲン捕捉剤等としての用途が期待される。
【０００４】
【課題を解決するための手段】
本発明によれば、前記本発明の目的は、生石灰を水中にて反応（消化反応）せしめて水酸化カルシウム粒子を製造する方法において、含水二酸化珪素を添加剤として含有する水中にて該消化反応を行うことを特徴とする水酸化カルシウム粒子の製造方法により達成される。
【０００５】
かかる本発明の方法により、ＢＥＴ比表面積が５〜４０ｃｍ２／ｇ、好ましくは２０〜４０ｍ２／ｇ、さらに好ましくは３０〜４０ｍ ２ ／ｇの高比表面積を有する水酸化カルシウム粒子が得られる。また得られた水酸化カルシウム粒子は、レーザ光回折散乱法による粒子径測定法に基づいて平均２次粒子径が２〜１０μｍ、好ましくは２．５〜８μｍである。
【０００６】
以下本発明方法についてさらに具体的に説明する。
【０００７】
本発明の方法は、含水二酸化珪素を添加剤として含有する水中にて生石灰（酸化カルシウム）を消化反応させる。好適には前記添加物を含有し、１０〜６０℃、好ましくは３０〜６０℃の水中に攪拌下に生石灰を供給して消化反応させる。反応温度は、生石灰を加えることによって自生熱により上昇し、例えば９０℃以上に達する。
【０００８】
消化反応中に含有される添加物は含水二酸化珪素である。
【０００９】
本発明の方法において、前記した添加物の使用量は、生成する水酸化カルシウム粒子に対して０．１〜２モル％、好適には０.２〜１.０モル％、さらに好適には０．５〜１ . ０モル％が有利である。０．１モル％より少ないと結晶成長阻害剤としての効果が小さくなくなり、生成する水酸化カルシウム粒子の比表面積が小さくなる。２.０モル％を超えると、Ｃａ−Ｓｉ、Ｃａ−Ａｌ、Ｃａ−Ｐなどの化合物および無機酸Ｃａ、有機酸Ｃａが生成すると共に、生成する水酸化カルシウム粒子中のカルシウム含量が少なくなり純度のよい目的物質を得ることが困難となる。
【００１０】
本発明の方法において、前記添加剤がどのような作用により水酸化カルシウム粒子のＢＥＴ表面積を大きくすることを可能としているのかは明らかではないが、添加剤が結晶成長阻害剤として働き結晶成長を制御するためと思われる。
【００１１】
本発明の方法により前述した消化反応を実施することにより、高比表面積を有する水酸化カルシウム粒子を得ることができるが、消化反応後さらに反応混合物を熟成することによって、さらに高品質の水酸化カルシウム粒子を得ることができる。この熟成は反応混合物を６０〜１７０℃、好ましくは８０〜１２０℃、最も好ましくは９０〜１００℃の温度で、５分〜３時間、好ましくは１０分〜２時間、より好ましくは２０分〜１時間実施することができる。
【００１２】
さらに反応終了後、もしくは熟成終了後、必要に応じて得られた水酸化カルシウム粒子を懸濁液中にて湿式ボールミルなどの粉砕手段で粉砕することもできる。粉砕することによって平均２次粒径が２μｍより小さい粒子を得ることができる。
【００１３】
本発明の方法により得られた水酸化カルシウム粒子は、所望により、それ自体公知の表面処理剤、例えばアニオン系界面活性剤により、表面処理することもできる。表面処理により、樹脂等への相溶性を改良することができる。
【００１４】
本発明者らの研究によれば、水酸化アルカリ金属と水溶性カルシウムとの反応時に本発明の添加剤を利用することも可能であることが判明した。すなわち、水酸化アルカリ金属に含水二酸化珪素を添加剤として添加しておき攪拌下、水溶性のカルシウム塩を加えて反応することもできる。反応後、必要に応じて熟成する方法により目的の水酸化カルシウム粒子が得られる。しかしながら、この製造方法は原料が高価であることさらに副生溶解質を洗浄により除く必要があるので経済性において劣る。
【００１５】
さらに本発明者らの研究によれば、一般的に実施されている生石灰を水に投入し消化反応して得られる水酸化カルシウム粒子懸濁液に、含水二酸化珪素を添加し、熟成により目的物質を得ることも可能であることが判明したがその効果が弱く有用性において劣る（参考例参照）。
【００１６】
【実施例】
以下、実施例を掲げて本発明を詳述する。
【００１７】
実施例１〜３
３Ｌ容ビーカーに水道水１．５リットルおよび添加剤として、塩野義製薬株式会社製含水二酸化珪素（カープレックス＃８０、ＳｉＯ２含量９５％）を、水酸化カルシウム粒子の収量の０.２モル％、０.５モル％または１.０モル％ に相当する量、それぞれ、０.５ｇ、１.３ｇまたは２.５ｇを入れ水温を約６０℃に昇温後、生石灰（ウベマテリアルズ株式会社製カルシード）２２５ｇを攪拌下に投入し消化反応せしめた。その後、９０℃で３０分間撹拌した（反応温度は９０℃以上に自生熱で上昇する。）。冷却後、２００メッシュの篩を通過し、濾過、脱水、乾燥、粉砕した。得られた粉末のＢＥＴ比表面積およびレーザ光回折散乱法粒度分布測定機で測定した２次粒子の平均粒子径を表１に示す。
【００１８】
比較例１
実施例２において、添加剤として協和化学工業株式会社製乾燥水酸化アルミニウムゲル（Ｓ−１００、Ａｌ含量２８.６％ ）とした以外は実施例２と同様に処理した。得られた粉末のＢＥＴ比表面積およびレーザ光回折散乱法粒度分布測定機で測定した２次粒子の平均粒子径を表１に示す。
【００１９】
比較例２
実施例２において、添加剤としてオルガノ株式会社製ポリリン酸ナトリウムとした以外は実施例２と同様に処理した。得られた粉末のＢＥＴ比表面積およびレーザ光回折散乱法粒度分布測定機で測定した２次粒子の平均粒子径を表１に示す。
【００２０】
比較例３および４
実施例２において、添加剤として、塩酸または硝酸とする以外は実施例２と同様に処理した。得られた粉末のＢＥＴ比表面積およびレーザ光回折散乱法粒度分布測定機で測定した２次粒子の平均粒子径を表１に示す。
【００２１】
比較例５〜８
実施例２および３において、添加剤として、クエン酸ナトリウムまたは酒石酸とする以外は実施例２および３と同様に処理した。得られた粉末のＢＥＴ比表面積およびレーザ光回折散乱法粒度分布測定機で測定した２次粒子の平均粒子径を表１に示す。
【００２２】
実施例４および５
実施例２および３の含水二酸化珪素０.５モル％および１.０モル％添加で得られた水酸化カルシウム懸濁液を、容量１Ｌのオートクレーブに入れ１２０℃で２時間水熱処理を行なった。冷後、２００メッシュの篩を通過し、濾過、脱水、乾燥、粉砕した。得られた粉末のＢＥＴ比表面積およびレーザ光回折散乱法粒度分布測定機で測定した２次粒子の平均粒子径を表１に示す。
【００２３】
実施例６および比較例９
実施例２の含水珪素０.５モル％および比較例６のクエン酸ナトリウム０.５モル％添加で得られた水酸化カルシウム懸濁液を８０℃に昇温後、攪拌下に、５％ステアリン酸ソーダー液（８０℃）を加えて表面処理を行なった。冷却後、２００メッシュの篩を通過し、濾過、脱水、乾燥、粉砕した。なお、ステアリン酸ソーダー添加量は水酸化カルシウム表面を単分子層で覆える量とした。得られた粉末のＢＥＴ比表面積およびレーザ光回折散乱法粒度分布測定機で測定した２次粒子の平均粒子径を表１に示す。
【００２４】
実施例７
実施例２の含水珪素０.５モル％添加で得られた水酸化カルシウム懸濁液を、湿式ボールミルとして、シンマルエンタープライゼス製ダイノ−ミルを用いて、ガラスビーズ径０.５ｍｍ、ディスク周速１０ｍ／ｓ、スラリー供給量２５０Ｌ／ｈの条件で粉砕し、濾過、脱水、乾燥、粉砕した。得られた粉末のＢＥＴ比表面積およびレーザ光回折散乱法粒度分布測定機で測定した２次粒子の平均粒子径を表１に示す。
【００２５】
実施例８〜１０
実施例１〜３において、消化反応終了後の熟成（９０℃で３０分撹拌する）をしないこと以外実施例１〜３と同様に処理した。得られた粉末のＢＥＴ比表面積およびレーザ光回折散乱法粒度分布測定機で測定した２次粒子の平均粒子径を表１に示す。
【００２６】
比較例１０
３Ｌ容ビーカーに水道水１．５リットルを入れ水温を約６０℃に昇温後、攪拌下に、生石灰２２５ｇを投入し消化反応する。その後、９０℃で３０分間攪拌した（反応温度は９０℃以上に自生熱で昇温する。）。冷却後、２００メッシュの篩を通過さし、濾過、脱水、乾燥、粉砕した。得られた粉末のＢＥＴ比表面積、レーザ回折法粒度分布測定機で測定した２次粒子の平均粒子径を表１に示す。
【００２７】
参考例
３Ｌ容ビーカーに水道水１．５リットルを入れ、水温を約６０℃に昇温後、撹拌下に、生石灰２２５ｇを投入し消化反応する。得られた水酸化カルシウム水溶液に、珪素系化合物として塩野義製薬株式会社製含水二酸化珪素（カープレックス＃８０，ＳｉＯ２含量９５％）を、水酸化カルシウム収量の０.５モル％に相当する量を添加し、９０℃で３０分間撹拌した。冷後、２００メッシュの篩を通過し、濾過、脱水、乾燥、粉砕した。得られた粉末のＢＥＴ比表面積およびレーザ光回折散乱法粒度分布測定機で測定した２次粒子の粒子径を表１に示す。
【００２８】
【表１】
【発明の効果】
本発明方法によれば、高比表面積を有する水酸化カルシウム粒子が容易に得られる。得られた水酸化カルシウム粒子は、比表面積が大きいので高活性であることにより酸中和剤やハロゲン捕捉剤等としての用途が期待される。さらに、反応は生石灰の消化を利用するので熱エネルギーは自生熱でまかなえることができ安価に、また、簡便に製造できる。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a method for producing calcium hydroxide particles having a high specific surface area. More specifically, the present invention relates to a method for producing calcium hydroxide particles having a high specific surface area that is high performance, simple and economical.
[0002]
[Prior art]
Calcium hydroxide particles are generally manufactured by a method in which quick lime (calcium oxide) is reacted with water. However, calcium hydroxide particles having a small specific surface area are easily grown due to high solubility of quick lime in water. Generate. Japanese Patent Application Laid-Open No. 2001-123071 describes a method in which a water-soluble calcium salt aqueous solution is poured into an aqueous solution containing an alkali metal hydroxide equivalent to or more than calcium to cause the reaction to age. However, the above method has a problem that the raw material is expensive and the by-product solute needs to be washed with water, and the produced particles are fine particles, which makes filtration difficult. Further, a sufficiently high specific surface area has not been obtained.
[0003]
[Problems to be solved by the invention]
An object of the present invention is to provide a method for easily and economically producing calcium hydroxide having a high specific surface area by overcoming the problems in the conventional method for producing calcium hydroxide particles. The calcium hydroxide particles according to the method of the present invention are highly active due to their large specific surface area, and are expected to be used as acid neutralizers, halogen scavengers and the like.
[0004]
[Means for Solving the Problems]
According to the present invention, the object of the present invention is to produce calcium hydroxide particles by reacting quicklime in water (digestion reaction), and in the water containing hydrous silicon dioxide as an additive , the digestion reaction Is achieved by a method for producing calcium hydroxide particles.
[0005]
The method of the present invention, BET specific surface area of 5~40cm 2 / g, preferably 20 to 40 m 2 / g, more preferably calcium hydroxide particles having a high specific surface area of 30 to 40 m 2 / g is obtained. The obtained calcium hydroxide particles have an average secondary particle size of 2 to 10 μm, preferably 2.5 to 8 μm, based on a particle size measurement method by a laser diffraction diffraction method.
[0006]
Hereinafter, the method of the present invention will be described more specifically.
[0007]
In the method of the present invention, quick lime (calcium oxide) is digested in water containing hydrous silicon dioxide as an additive . Suitably, the additive is contained, and quick lime is supplied to water at 10 to 60 ° C., preferably 30 to 60 ° C. with stirring, to cause a digestion reaction. The reaction temperature rises due to autogenous heat by adding quicklime, and reaches, for example, 90 ° C. or more.
[0008]
The additive contained during the digestion reaction is hydrous silicon dioxide.
[0009]
In the method of the present invention, the amount of the additive used is 0.1 to 2 mol%, preferably 0.2 to 1.0 mol% , more preferably 0, based on the calcium hydroxide particles produced. .5～1. 0 mol% are advantageous. When the amount is less than 0.1 mol%, the effect as a crystal growth inhibitor is not reduced, and the specific surface area of the generated calcium hydroxide particles is reduced. If it exceeds 2.0 mol%, compounds such as Ca-Si, Ca-Al, and Ca-P, inorganic acid Ca, and organic acid Ca are produced, and the calcium content in the produced calcium hydroxide particles is reduced and purity. It is difficult to obtain a good target substance.
[0010]
In the method of the present invention, it is not clear what effect the additive can increase the BET surface area of the calcium hydroxide particles, but the additive acts as a crystal growth inhibitor to control crystal growth. It seems to do.
[0011]
By carrying out the above-described digestion reaction by the method of the present invention, calcium hydroxide particles having a high specific surface area can be obtained. By aging the reaction mixture after the digestion reaction, higher quality calcium hydroxide can be obtained. Particles can be obtained. This aging is performed at a temperature of 60 to 170 ° C., preferably 80 to 120 ° C., most preferably 90 to 100 ° C. for 5 minutes to 3 hours, preferably 10 minutes to 2 hours, more preferably 20 minutes to 1 ° C. Can be implemented for hours.
[0012]
Furthermore, after completion of the reaction or after completion of aging, the calcium hydroxide particles obtained may be pulverized in a suspension by a pulverizing means such as a wet ball mill. By pulverizing, particles having an average secondary particle size of less than 2 μm can be obtained.
[0013]
If desired, the calcium hydroxide particles obtained by the method of the present invention can be surface-treated with a surface treatment agent known per se, for example, an anionic surfactant. The surface treatment can improve compatibility with a resin or the like.
[0014]
According to the studies by the present inventors, it has been found that the additive of the present invention can also be used during the reaction between an alkali metal hydroxide and water-soluble calcium. That is, hydrous silicon dioxide can be added as an additive to an alkali metal hydroxide, and a water-soluble calcium salt can be added and reacted with stirring. After the reaction, target calcium hydroxide particles are obtained by a method of aging as necessary. However, this production method is inferior in economic efficiency because the raw material is expensive and the by-product solute needs to be removed by washing.
[0015]
Furthermore, according to the study by the present inventors, water-containing silicon dioxide is added to a calcium hydroxide particle suspension obtained by digestion reaction by adding quick lime which is generally carried out to water, and the target substance is obtained by aging. However, the effect is weak and the utility is inferior (see Reference Example).
[0016]
【Example】
Hereinafter, the present invention will be described in detail with reference to examples.
[0017]
Examples 1-3
In a 3 L beaker, 1.5 liters of tap water and hydrous silicon dioxide (Carplex # 80, SiO 2 content 95%) manufactured by Shionogi & Co., Ltd. as an additive , 0.2 mol% of the yield of calcium hydroxide particles. , 0.5 mol% or 1.0 mol%, and 0.5g, 1.3g or 2.5g, respectively, and after raising the water temperature to about 60 ° C, quick lime (manufactured by Ube Materials Co., Ltd.) 225 g of calcede) was added under stirring to cause a digestion reaction. Thereafter, the mixture was stirred at 90 ° C. for 30 minutes (the reaction temperature rose to 90 ° C. or more by autogenous heat). After cooling, it passed through a 200-mesh sieve, filtered, dehydrated, dried and pulverized. Table 1 shows the BET specific surface area of the obtained powder and the average particle diameter of secondary particles measured with a laser light diffraction / scattering particle size distribution analyzer.
[0018]
Comparative Example 1
In Example 2 , it processed like Example 2 except having set it as dry additive aluminum hydroxide gel (S-100, Al content 28.6%) by Kyowa Chemical Industry Co., Ltd. as an additive . Table 1 shows the BET specific surface area of the obtained powder and the average particle diameter of secondary particles measured with a laser light diffraction / scattering particle size distribution analyzer.
[0019]
Comparative Example 2
In Example 2 , it processed like Example 2 except having set it as sodium polyphosphate by Organo Corporation as an additive . Table 1 shows the BET specific surface area of the obtained powder and the average particle diameter of secondary particles measured with a laser light diffraction / scattering particle size distribution analyzer.
[0020]
Comparative Examples 3 and 4
In Example 2 , the same treatment as in Example 2 was performed except that hydrochloric acid or nitric acid was used as an additive . Table 1 shows the BET specific surface area of the obtained powder and the average particle diameter of secondary particles measured with a laser light diffraction / scattering particle size distribution analyzer.
[0021]
Comparative Examples 5-8
In Examples 2 and 3 , the same treatment as in Examples 2 and 3 was conducted except that sodium citrate or tartaric acid was used as an additive . Table 1 shows the BET specific surface area of the obtained powder and the average particle diameter of secondary particles measured with a laser light diffraction / scattering particle size distribution analyzer.
[0022]
Examples 4 and 5
The calcium hydroxide suspensions obtained by adding 0.5 mol% and 1.0 mol% of the hydrous silicon dioxide of Examples 2 and 3 were placed in a 1 L autoclave and hydrothermally treated at 120 ° C. for 2 hours. After cooling, it passed through a 200-mesh sieve, filtered, dehydrated, dried and pulverized. Table 1 shows the BET specific surface area of the obtained powder and the average particle diameter of secondary particles measured with a laser light diffraction / scattering particle size distribution analyzer.
[0023]
Example 6 and Comparative Example 9
The calcium hydroxide suspension obtained by adding 0.5 mol% of hydrous silicon in Example 2 and 0.5 mol% of sodium citrate in Comparative Example 6 was heated to 80 ° C. and then stirred with 5% stearin. A surface treatment was performed by adding an acid soda solution (80 ° C.). After cooling, it passed through a 200-mesh sieve, filtered, dehydrated, dried and pulverized. The amount of sodium stearate added was such that the surface of calcium hydroxide was covered with a monomolecular layer. Table 1 shows the BET specific surface area of the obtained powder and the average particle diameter of secondary particles measured with a laser light diffraction / scattering particle size distribution analyzer.
[0024]
Example 7
The calcium hydroxide suspension obtained by adding 0.5 mol% of hydrous silicon in Example 2 was used as a wet ball mill using a Dyno mill made by Shinmaru Enterprises, with a glass bead diameter of 0.5 mm and a disk peripheral speed. The mixture was pulverized under conditions of 10 m / s and a slurry supply amount of 250 L / h, filtered, dehydrated, dried and pulverized. Table 1 shows the BET specific surface area of the obtained powder and the average particle diameter of secondary particles measured with a laser light diffraction / scattering particle size distribution analyzer.
[0025]
Examples 8-10
In Examples 1-3 , it processed like Examples 1-3 except not carrying out the ageing | curing | ripening after completion | finish of digestion reaction (it stirs at 90 degreeC for 30 minutes). Table 1 shows the BET specific surface area of the obtained powder and the average particle diameter of secondary particles measured with a laser light diffraction / scattering particle size distribution analyzer.
[0026]
Comparative Example 10
After putting 1.5 liters of tap water in a 3 L beaker and raising the water temperature to about 60 ° C., 225 g of quick lime is added and a digestion reaction is performed with stirring. Thereafter, the mixture was stirred at 90 ° C. for 30 minutes (reaction temperature was raised to 90 ° C. or higher by autogenous heat). After cooling, the mixture was passed through a 200-mesh sieve, filtered, dehydrated, dried and pulverized. Table 1 shows the BET specific surface area of the obtained powder and the average particle diameter of secondary particles measured with a laser diffraction particle size distribution analyzer.
[0027]
Reference Example 1.5 liters of tap water is put into a 3 L beaker, and after raising the water temperature to about 60 ° C., 225 g of quick lime is added with stirring to cause a digestion reaction. To the obtained aqueous calcium hydroxide solution, hydrous silicon dioxide (Carplex # 80, SiO 2 content 95%) manufactured by Shionogi & Co., Ltd. as a silicon compound is added in an amount corresponding to 0.5 mol% of the calcium hydroxide yield. And stirred at 90 ° C. for 30 minutes. After cooling, it passed through a 200-mesh sieve, filtered, dehydrated, dried and pulverized. Table 1 shows the BET specific surface area of the obtained powder and the particle diameter of secondary particles measured by a laser light diffraction / scattering particle size distribution analyzer.
[0028]
[Table 1]
【The invention's effect】
According to the method of the present invention, calcium hydroxide particles having a high specific surface area can be easily obtained. Since the obtained calcium hydroxide particles have a large specific surface area, they are expected to be used as acid neutralizers, halogen scavengers and the like due to their high activity. Furthermore, since the reaction uses digestion of quicklime, the heat energy can be covered by the self-generated heat, and can be manufactured inexpensively and simply.
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| JP4775950B2 (en) * | 2003-11-13 | 2011-09-21 | 協和化学工業株式会社 | Resin composition and molded article containing calcium hydroxide |
| JP4606238B2 (en) * | 2005-04-25 | 2011-01-05 | 株式会社トクヤマ | Method for producing calcium hydroxide slurry |
| JP5348886B2 (en) * | 2005-04-28 | 2013-11-20 | 協和化学工業株式会社 | Resin composition |
| JP2016128382A (en) * | 2016-02-18 | 2016-07-14 | 古手川産業株式会社 | Hydrated lime and acid gas remover |
| CN110407559A (en) * | 2019-07-30 | 2019-11-05 | 南京信息工程大学 | A kind of modified haydite and its application |
| CN112358205A (en) * | 2020-11-27 | 2021-02-12 | 广西合山市华纳新材料科技有限公司 | Preparation method of high-activity calcium hydroxide |
| CN113666405B (en) * | 2021-08-11 | 2023-03-31 | 襄阳兴发化工有限公司 | Preparation method of high-specific-surface-area and high-whiteness calcium hydroxide |
| CN114538799B (en) * | 2021-10-18 | 2022-09-13 | 浙江天石纳米科技股份有限公司 | Preparation method of calcium hydroxide powder with cluster-shaped meristematic structure and ultra-high specific surface area |
| CN116903270B (en) * | 2023-09-06 | 2023-12-05 | 山东万达环保科技有限公司 | Preparation method of calcium hydroxide with high specific surface area |
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